CN102557626A - Preparation method of honeycomb-structure spherical powder material for rare earth modified zirconia thermal barrier coating - Google Patents
Preparation method of honeycomb-structure spherical powder material for rare earth modified zirconia thermal barrier coating Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 75
- 239000000463 material Substances 0.000 title claims abstract description 44
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- -1 rare earth modified zirconia Chemical class 0.000 title claims abstract description 20
- 239000012720 thermal barrier coating Substances 0.000 title abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 15
- 238000000280 densification Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 238000000975 co-precipitation Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001694 spray drying Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910052726 zirconium Inorganic materials 0.000 claims abstract 2
- 238000000576 coating method Methods 0.000 claims description 33
- 239000011248 coating agent Substances 0.000 claims description 32
- 230000004888 barrier function Effects 0.000 claims description 26
- 239000012254 powdered material Substances 0.000 claims description 20
- 230000001413 cellular effect Effects 0.000 claims description 19
- 238000005507 spraying Methods 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000003483 aging Methods 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 3
- 239000002585 base Substances 0.000 claims 3
- 239000003518 caustics Substances 0.000 claims 3
- 239000007788 liquid Substances 0.000 claims 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims 1
- 206010013786 Dry skin Diseases 0.000 claims 1
- 229910052692 Dysprosium Inorganic materials 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052693 Europium Inorganic materials 0.000 claims 1
- 229910052779 Neodymium Inorganic materials 0.000 claims 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
- 229910052772 Samarium Inorganic materials 0.000 claims 1
- 229910052769 Ytterbium Inorganic materials 0.000 claims 1
- BNUDRLITYNMTPD-UHFFFAOYSA-N acetic acid;zirconium Chemical compound [Zr].CC(O)=O BNUDRLITYNMTPD-UHFFFAOYSA-N 0.000 claims 1
- 230000029087 digestion Effects 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 229910052746 lanthanum Inorganic materials 0.000 claims 1
- 150000002823 nitrates Chemical class 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 claims 1
- 238000005469 granulation Methods 0.000 abstract description 5
- 230000003179 granulation Effects 0.000 abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 abstract description 5
- 230000032683 aging Effects 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 2
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 2
- 239000007767 bonding agent Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 229910000420 cerium oxide Inorganic materials 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 5
- RFNWHNKWWHCSGS-UHFFFAOYSA-N [O-2].[Y+3].[O-2].[Ce+3] Chemical compound [O-2].[Y+3].[O-2].[Ce+3] RFNWHNKWWHCSGS-UHFFFAOYSA-N 0.000 description 4
- 230000002950 deficient Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000007669 thermal treatment Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- BHXBZLPMVFUQBQ-UHFFFAOYSA-K samarium(iii) chloride Chemical compound Cl[Sm](Cl)Cl BHXBZLPMVFUQBQ-UHFFFAOYSA-K 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910002076 stabilized zirconia Inorganic materials 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
本发明提供了一种稀土改性氧化锆热障涂层用蜂窝状结构球形粉末材料及其制备方法，通过采用前驱体直接团聚制粒-烧结致密化的工艺合成稀土改性蜂窝状结构粉末材料。包括将稀土元素与锆元素按照预定重量比例与水混合制成水溶液，加入碱液调节溶液pH值，使水溶液发生共沉淀反应，将白色沉淀陈化数小时得到前驱体凝胶；对前驱体凝胶使用预定介质进行洗涤，直到用硝酸银检测不到氯离子为止；将洗涤后的前驱体凝胶与预定介质按照一定比例进行混合获得混合溶液，向混合溶液中加入适量的分散剂和粘结剂，调制出适用于可控蜂窝状多孔结构的料浆配方，再通过喷雾干燥将浆料制成团聚粉末材料；对团聚粉末材料进行预定时间的致密化处理后，制得蜂窝状结构的球形粉末材料；制备的粉末具有高松装密度、良好流动性等特点，粉末的微观组织为布满均匀孔隙的蜂窝状结构。
The invention provides a honeycomb structure spherical powder material for rare earth modified zirconia thermal barrier coatings and a preparation method thereof. The rare earth modified honeycomb structure powder material is synthesized by adopting the process of direct agglomeration, granulation and sintering densification of the precursor . It includes mixing rare earth elements and zirconium elements with water according to a predetermined weight ratio to make an aqueous solution, adding lye to adjust the pH value of the solution, causing a co-precipitation reaction in the aqueous solution, aging the white precipitate for several hours to obtain a precursor gel; The gel is washed with a predetermined medium until no chloride ions are detected with silver nitrate; the washed precursor gel is mixed with the predetermined medium according to a certain ratio to obtain a mixed solution, and an appropriate amount of dispersant and bonding agent are added to the mixed solution. Prepare a slurry formula suitable for a controllable honeycomb porous structure, and then make the slurry into an agglomerated powder material by spray drying; after densifying the agglomerated powder material for a predetermined time, a spherical honeycomb structure can be obtained Powder material; the prepared powder has the characteristics of high bulk density and good fluidity, and the microstructure of the powder is a honeycomb structure covered with uniform pores.
Description
Technical field
The present invention relates to the preparation method of a kind of rare earth modified Zirconium oxide heat barrier coating, belong to field of material preparation with the polynuclear plane spherical powder material.
Background technology
Along with the direction of turbine engine to high flow capacity ratio, high thrust-weight ratio develops, the Service Environment of the high-temperature component of mover is harsh more.Thrust-weight ratio is that the design inlet temperature of 10 aircraft engine has reached 1600-1700 ℃, and existing high temperature alloy and cooling technology are difficult to satisfy the design requirements of modern aeroengine.People begin to attempt using thermal barrier coating (TBCs) technology further to improve the working temperature of mover.Thermal barrier coating is exactly that this coating has the metallic matrix of reduction heating temperature, prevents the matrix alloy oxidation, guarantees these parts works better under higher relatively temperature at the resistant to elevated temperatures material with low thermal conductivity of the surface of component spraying one deck.Be mainly used in various high-temperature heat engines; Like the rotor of internal combustion turbine or jet plane or the surperficial heat insulating coat of stator vane, engine combustion chamber interior walls, gasoline or diesel combustion chamber interior walls; Rocket nozzle; Or some other high-temp combustion device inwall, perhaps heat insulation, the inoxidzable coating material of the metallic element of a few thing under hot environment can effectively prolong the work-ing life of hot-end component and the efficient of raising internal combustion turbine.
Present widely used thermal barrier coating mainly is that employing quality percentage composition is 6-8wt% yttrium oxide (Y
2O
3) PSZ (ZrO
2) material (being called for short YSZ).But; YSZ recycles in the process under being higher than 1200 ℃ of temperature for a long time, and coated material exists phase transformation, grain growth, little pore to shrink phenomenons such as sintering, makes thermal conductivity increase; The interface thermal stresses raises and causes disbonding, causes hot machine to reduce work-ing life.And REE has higher chemicalstability, and high melt point is at ZrO
2In can limited solid solution, rare earth modified ZrO
2Material crystals inside has than the more room of YSZ, more complicated cell configuration; And contain the bigger rare earth atom of quality in the structure cell; Thereby increased the scattering of phonon greatly, cause the mfp of phonon to reduce, thereby make material thermal conductivity lower than YSZ.And under appropriate proportioning, can give full play to the excellent lattice stabilization of rare earth heavy ion radius, make and adopt rare earth codoped ZrO
2The coating of material prepn; Can keep mutually stable more than 1200 ℃ for a long time; Have good thermal shock resistance simultaneously, satisfy more abominable work condition environment, the existence of specific rare earth oxide can be played good catalyst catalysis and the effect that reduces exhaust gas emission in addition.Therefore, rare earth modified zirconia of heat barrier coat material be a kind of have an applications well prospect be used for the high-temperature fuel gas turbine, high-temperature heat engines such as turbo-jet engine are used the new type high temperature heat barrier coat material.
And prepare rare earth modified Zirconium oxide heat barrier coating powdered material at present, mostly for solid construction or be applicable to the hollow structure that can wear and tear application.Density is higher, the thermal barrier coating powdered material of solid construction be difficult for to melt in spraying process, but powder inside do not melt block and in coating structure, forms the defective source, causes the coating inefficacy.The powdered material loose density of hollow structure is lower, is prone to cause flying away of powder in the spraying process, and not only powder utilization is low, and there are defectives such as hole is bigger in the coating of preparation.
And the thermal barrier coating powder inside of polynuclear plane has been covered with a large amount of micro-pores, and the thawing of powder is respond well, possesses suitable loose density, and the spraying coating process window is more wide in range.And can prepare the coating of even dispersion microvoid structure, reduce the coating structure defective, make the inner stress of coating obtain discharging and alleviating, effectively promote the thermal shock resistance of coating.The last employing of preparation method chemical coprecipitation synthesizes the zirconia of heat barrier coat material presoma, can effectively ensure the homodisperse of each component.Adopt rational slip prescription, utilize presoma to carry out directly that slurry is synthetic, the method for agglomeration granulation, prepare the presoma reunion powder of vesicular structure, dehydration reaction generation ZrO takes place in powder in sintering process on the one hand
2,, be prone to realize the low-temperature sintering of powder owing to need heat lower; On the other hand; The powder dehydration reaction is accompanied by the hard aggregation process of old bond rupture, new key formation, when keeping honey-combed, causes the powder volume contraction; Bonding force strengthens between the powder endoparticle, has effectively guaranteed the honeycomb vesicular structure intensity of powder and than high apparent density.
Summary of the invention
The present invention for solve that the rare earth modified Zirconium oxide heat barrier coating powdered material technology of existing preparation exists when the employing solid construction; Do not melt block because of inside and in coating structure, form the defective source, thereby cause coating to lose efficacy, and when adopting hollow structure; The powdered material loose density is lower; Be prone to cause flying away of powder in the spraying process, not only powder utilization is low, and there are problems such as hole is bigger in the coating of preparation; The preparation method of a kind of rare earth modified Zirconium oxide heat barrier coating with the polynuclear plane spherical powder material is provided, comprised:
Step 1; With the salt of REE and salt or the compound of REE and the compound of zr element of zr element; Be mixed and made into the aqueous solution according to predetermined weight ratio and water, in the said aqueous solution, add alkali lye regulator solution pH value, make said aqueous solution generation coprecipitation reaction; And constantly stir until forming white precipitate, said white precipitate ageing number hour is obtained aqueous precursor gel;
Step 3; Said aqueous precursor gel after the washing is mixed the acquisition mixing solutions according to a certain percentage with predetermined medium; In said mixing solutions, add an amount of dispersion agent and sticker; And disperse to be mixed with slurry in 1～30 hour through ball milling and ultrasonic vibration, through spraying drying said slurry is processed the reunion powder material again;
Step 4, said reunion powder material carried out densification after, make the spherical powder material of cellular porous structure;
Step 5 is sieved said powdered material, and the rare earth modified Zirconium oxide heat barrier coating that obtains the predetermined particle size scope is used the polynuclear plane spherical powder material.
The rare earth modified Zirconium oxide heat barrier coating of cellular porous structure provided by the invention is with polynuclear plane spherical powder material and preparation technology thereof; For the heat barrier coat material of traditional preparation process; Have cellular porous structure through adopting the preparation technology of the synthetic presoma of chemical coprecipitation and the granulations-sintering densification of directly reuniting, can preparing, good sphericity, high apparent density, composition uniformity coefficient and the high temperature rare earth modified Zirconium oxide heat barrier coating powder of maintenance good stability down.
Description of drawings
Fig. 1 is the schematic flow sheet of the rare earth modified Zirconium oxide heat barrier coating that provides of the specific embodiment of the invention with the preparation method of polynuclear plane spherical powder material;
Fig. 2 is the microstructure synoptic diagram of the cerium oxide with cellular porous structure-yttrium oxide co-stabilized Zirconium oxide heat barrier coating reunion powder of providing of the specific embodiment of the invention.
Fig. 3 is the diagrammatic cross-section of the cerium oxide with cellular porous structure-yttrium oxide co-stabilized Zirconium oxide heat barrier coating reunion powder of providing of the specific embodiment of the invention.
Fig. 4 is the minimum crystal grain TEM figure in the cerium oxide with cellular porous structure-yttrium oxide co-stabilized Zirconium oxide heat barrier coating powder agglomerates of providing of the specific embodiment of the invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is carried out clear, intactly description, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on embodiments of the invention, those of ordinary skills belong to protection scope of the present invention not making the every other embodiment that is obtained under the creative work prerequisite.
Embodiment of the present invention provides the preparation method of a kind of rare earth modified Zirconium oxide heat barrier coating with the polynuclear plane spherical powder material, and is as shown in Figure 1, comprising:
Step 1; With the salt of REE and salt or the compound of REE and the compound of zr element of zr element; Be mixed and made into the aqueous solution according to predetermined weight ratio and water, in the said aqueous solution, add alkali lye regulator solution pH value, make said aqueous solution generation coprecipitation reaction; And constantly stir until forming white precipitate, said white precipitate ageing number hour is obtained aqueous precursor gel;
Step 3; Said aqueous precursor gel after the washing is mixed the acquisition mixing solutions according to a certain percentage with predetermined medium; In said mixing solutions, add an amount of dispersion agent and sticker; And disperse to be mixed with slurry in 1～30 hour through ball milling and ultrasonic vibration, through spraying drying said slurry is processed the reunion powder material again;
Step 4, said reunion powder material carried out densification after, make the spherical powder material of cellular porous structure;
Step 5 is sieved said powdered material, and the rare earth modified Zirconium oxide heat barrier coating that obtains the predetermined particle size scope is used the polynuclear plane spherical powder material.
To combine the Figure of description specific embodiments of the invention to do to describe in detail further below.
Embodiment 1:
Be used to produce the preparation method of the spherical cerium oxide-yttrium oxide co-stabilized Zirconium oxide heat barrier coating powdered material of cellular porous structure; Comprise the following steps: to get 100kg zirconium oxychloride, 1.55kg Yttrium trichloride crystal powder and 27.52Kg Cerium II Chloride crystal powder; Add the 595kg deionized water, evenly stir and obtain uniform solution.To add concentration be 40% ammonia soln 145kg the 70min time in solution, and co-precipitation obtains gel and carries out the 10h ageing and handle, and after the filtration washing press filtration, obtains the filter cake of about 715kg.Add 700kg water at 1: 1 according to weight ratio,, obtain uniform and stable slurry through stirring ball-milling 10h.
Adopt centrifugal spraying drying that uniform and stable slurry is carried out spray-drying process, inlet temperature is 320 ℃, and temperature out is 110 ℃, and centrifugal atomizing dish rotating speed is 11000r/min, and cyclonic separator is used to collect the powdered material after the granulation.With the powder 700 ℃ of following thermal treatment 3h in retort furnace after collecting, obtain the cerium oxide-yttrium oxide co-stabilized Zirconium oxide powder of the cellular porous structure of agglomerating.Through the atmospheric plasma densification, make later the instantaneous densification of rare earth modified Zirconium oxide powder of sintering, and collect through powder collection device.The groundwork medium that atmospheric plasma is handled is an argon gas, and temperature is 8000-10000 ℃, and power is 40kW, and powder sending quantity is 6kg/h.
Powder after the plasma densification is sieved (500 order) promptly obtain the cerium oxide of cellular porous structure-yttrium oxide co-stabilized zirconia powder powder material; This powder-product loose density is 2.0g/cm3; Flowability is 38s/50g; The powdered material average grain size is 50nm, has good high-temperature stability, and the micro-structure diagram of powder is as shown in Figure 2.
Embodiment 2:
Be used to produce the spherical gadolinium sesquioxide (Gd of cellular porous structure
2O
3) preparation method of stabilizing zirconia of heat barrier coat powdered material, comprise the following steps: to get 50kg zirconium oxychloride and 2.13Kg Gadolinium trinitrate crystal powder, add the 595kg deionized water, evenly stir and obtain uniform solution.To add concentration be 30% ammonia soln 145kg the 70min time in solution, and co-precipitation obtains gel and carries out the 10h ageing and handle, and after the filtration washing press filtration, obtains the filter cake of about 715kg.Add the 700kg deionized water at 1: 1 according to weight ratio,, obtain uniform and stable slurry through stirring ball-milling 12h.
Adopt centrifugal spraying drying that uniform and stable slurry is carried out spray-drying process, inlet temperature is 330 ℃, and temperature out is 130 ℃, and centrifugal atomizing dish rotating speed is 11000r/min, and cyclonic separator is used to collect the powdered material after the granulation.With the powder 800 ℃ of following thermal treatment 5h in retort furnace after collecting, obtain the gadolinium oxide-stabilized Zirconium oxide powder of the cellular porous structure of agglomerating.
The powder of sintering densification is sieved (500 order) promptly obtain the cerium oxide of cellular porous structure-yttria-stabilized zirconia ceramic powder material product; This powder-product loose density is 1.7g/cm3; Flowability is 42s/50g, and the powdered material average grain size is 90nm.
Embodiment 3:
Be used to produce the spherical Samarium trioxide (Sm of cellular porous structure
2O
3The preparation method of)-stabilizing zirconia of heat barrier coat powdered material comprises the following steps: to get 100kg zirconium oxychloride and 3.5Kg samarium trichloride crystal powder, adds the 610kg deionized water, evenly stirs and obtains uniform solution.To add concentration be 40% ammonia soln 145kg the 70min time in solution, and co-precipitation obtains gel and carries out the 10h ageing and handle, and after the filtration washing press filtration, obtains the filter cake of about 715kg.Add 700kg water at 1: 1 according to weight ratio, through stirring ball-milling 5h, ultrasonic dispersing 3h obtains uniform and stable slurry.
Adopt centrifugal spraying drying that uniform and stable slurry is carried out spray-drying process, inlet temperature is 340 ℃, and temperature out is 130 ℃, and centrifugal atomizing dish rotating speed is 11000r/min, and cyclonic separator is used to collect the powdered material after the granulation.With the powder 700 ℃ of following thermal treatment 5h in retort furnace after collecting, obtain the cerium oxide-yttrium oxide co-stabilized Zirconium oxide powder of the cellular porous structure of agglomerating.Through the atmospheric plasma spray gun, make later the instantaneous densification of yttrium oxide-stabilized zirconium oxide powder of sintering, and collect through powder collection device.The groundwork medium that atmospheric plasma is handled is an argon gas, and temperature is 8000-10000 ℃, and power is 38kW, and powder sending quantity is 5kg/h.
Powder after the plasma densification is sieved (500 order) obtain promptly that the cerium oxide-yttrium oxide of cellular porous structure is apt decides zirconia ceramics powdered material product, this powder-product loose density is 2.1g/cm
3, flowability is 34s/50g, the powdered material average grain size is 70nm.
The rare earth modified Zirconium oxide heat barrier coating of the cellular porous structure that this embodiment provides is with the preparation technology of powdered material; For the heat barrier coat material of traditional preparation process; Have cellular porous structure through adopting the preparation technology of the synthetic presoma of chemical coprecipitation and the granulations-sintering densification of directly reuniting, can preparing, high apparent density, composition are even, the high temperature rare earth modified Zirconium oxide heat barrier coating powder of maintenance good stability down.This method economy, environmental protection, be suitable for industrial large-scale production, be with a wide range of applications.
The above; Be merely the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (10)
1. a rare earth modified Zirconium oxide heat barrier coating is characterized in that with the preparation method of polynuclear plane spherical powder material, comprising:
Step 1; With the salt of REE and salt or the compound of REE and the compound of zr element of zr element; Be mixed and made into the aqueous solution according to predetermined weight ratio and water, in the said aqueous solution, add alkali lye regulator solution pH value, make said aqueous solution generation coprecipitation reaction; And constantly stir until forming white precipitate, said white precipitate ageing number hour is obtained aqueous precursor gel;
Step 2 uses predetermined medium to wash to said aqueous precursor gel, till detecting less than cl ions with Silver Nitrate;
Step 3; Said aqueous precursor gel after the washing is mixed the acquisition mixing solutions according to a certain percentage with predetermined medium; In said mixing solutions, add an amount of dispersion agent and sticker; And disperse to be mixed with slurry in 1～30 hour through ball milling and ultrasonic vibration, through spraying drying said slurry is processed the reunion powder material again;
Step 4, said reunion powder material carried out densification after, make the spherical powder material of cellular porous structure;
Step 5 is sieved said powdered material, and the rare earth modified Zirconium oxide heat barrier coating that obtains the predetermined particle size scope is used the polynuclear plane spherical powder material.
2. method according to claim 1; It is characterized in that; In step 1; Said REE is one or more among Ce, La, Pr, Nb, Nd, Dy, Sm, Gd, Yb, Eu, the Er, and the salt of said REE comprises one or more in muriate, oxide compound, carbonate, nitrate salt, acetate or the Citrate trianion, and the salt of said zr element comprises one or more in zirconium oxychloride, zirconium carbonate, sour slightly zirconium, zirconium chloride, the acetic acid zirconium; The compound of said REE accounts for 1～60% of raw material total mass, and it is 40～99% that the compound of said zr element accounts for mass ratio.
3. method according to claim 1; It is characterized in that said step 1 specifically comprises: the salt of REE and the solubility salt of zr element are mixed by mass ratio 1: 2～40 with water, add strong base solution liquid or weak caustic solution fast; The volumetric concentration of said strong base solution liquid or weak caustic solution is 10%～80%; The adding speed of said strong base solution liquid or weak caustic solution is 0.1～10kg/min, regulates pH value to 8～11, digestion time 2～12 hours.
4. method according to claim 1 is characterized in that, in step 2, the said medium that presoma is washed is water, alcohol or methyl alcohol.
5. method according to claim 1; It is characterized in that; In step 3, said dispersion agent is polyoxyethylene glycol, ROHM or SEPIGEL 305, and said sticker is PVA, PVP or CMC; The weight percentage of said dispersion agent in mixing solutions is 0～15%, and the weight percentage of said sticker in mixing solutions is 0～15%.
6. preparation method according to claim 1; It is characterized in that; In step 3; The said method of processing the reunion powder material comprises one or more in centrifugal spray drying, pressure spray dryer or the two streaming spraying dryings, and said spray-dired inlet temperature is 150～350 ℃, and temperature out is 70～250 ℃.
7. preparation method according to claim 1 is characterized in that, in step 4, the sintering temperature of said reunion powder material is 400～1200 ℃, and sintering time is 2～15 hours.
8. method according to claim 1 is characterized in that, in step 5, the reunion powder material ranges after the said screening is 15～120 μ m.
9. method according to claim 1; It is characterized in that; Said step 4 also comprises: handles through the atmospheric plasma spray gun, makes the instantaneous densification of the spherical agglomerated powdered material of polynuclear plane behind the sintering, and through the polynuclear plane reunion powder material after the powder collection device collection and treatment.
10. method according to claim 9 is characterized in that, in passing through atmospheric plasma spray gun treating processes, working medium is an argon gas, and temperature is 8000～12000 ℃, and power is 30～60KW, and powder sending quantity is 1～15kg/h.
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